Process of treating ores.



P. A. EMANUEL.

PROCESS OF TREATING ORES.

APPLIOATION rum) SEPT. 29, 1909.

57,756. Patented May 10, 1910.

2 SHEETS-SHEET 1.

nn Qnnnnn P. A. EMANUEL. PROCESS OF TREATING ORES. APPLICATIONI'ILEDSBP'T. 29, 1909. 957,756. Patented May 10, 1910.

2 SHEETS-SHEET 2.

P A. EMANUEL, OF AIKEN, SOUTH CAROLINA.

PROCESS .OF TREATIKQ OBES.

names.

Specification of letters Patent.

Patented m 1o, 19m.

Original application med May 28, 1909, Serial No. 499,202. Divided andthis appllcation flled September 29,

- 1909. Serial No. 880,21

I South Carolina, have invented certain new and useful Improvements inProcesses of- Treating Ores; and I do hereby declare the following to bea full, clear, and exact description of the invention, such as willenable others skilled in the art to which it appertains to make and usethe same.

My invention relates to processes of treating ores and is designed totreat ordinary clays in such a manner as to save all their valuableconstituents and at the same time make use of the by-products. It isalso applicable to the treatment of bauxite and corundu-m for the makingof soda, a double sulfate of sodium and aluminum, silica, aluminumfluorid, sodium sulfate, metallic sodium, and aluminate of sodium, thisapplication being a division of my former application, Serlal No.499,202, filed May 29, 1909.

I carry out my rocess by an apparatus a part of which is s ow-n in theaccompanying drawings, and in which-- Figure 1 is a side elevationshowing my invention. Fig. 2 is ahorizonta-l cross section thereof. Fig.3 is a cross section through the retort. Fi 4 is a side elevation on alarger scale, s owing part of the rctort'and part of the furnace, andFig. 5

is a partial section showing part of the retort and the manner ofsecuring the wire netting thereon.

Referrin to the drawings, A represents the retort, the furnace portion,and C the portion connecting the retort with the smoke stack.

The retort is composed of a cylindrical bodyedportion 1,.having at eachend an extend portion 2,.forming a flange on which the portion 3 isbolted. The part 3 is cylindrical, and open at both ends, but having oneend bent inwardly to embrace the portion 2, both ends of the retortbeing exactly similar.

4 represents a perforated 'plate fitting tightly against the end of theretort, a suitable packing 5 of asbestos or similar material being usedif desired. Bolts 6 pass through the bent-in end of the part 3 in cars13, projecting from the bod mentioned.

through the part 2 and through the plate 4, uniting the whole firmlytogether.

7 re "resents tubes which ass through the end p ates 4, the ends of wiich are secured in perforations in the plate 8, secured to the plate 4.

At the top and bottom the retort is prov1ded with curved doors 9, hingedthereto, and with two pipes 10, each provided with a cock, such as 11,screwed into the cover. Each of the doors is mounted on a rod 12, of theretort, and on the retort are mountcr "swinging bolts 14, adapted toswin down behind projections 15 on the cover, thus firmly looking thecovers in position. 'ihny desired means, however, may be adopted forfastening the covers to the retort. The top and bottom covers areprecisely similar.

14 represents a layer of asbestos, or similar refractory material,placed over the outer side of the retort, including the covers,

and held in place by the wire netting 15,

angular frame 19, by means of depending are firmly fastened to the parts3 by beingbolted thereto, or made integral therewith, and have theirupper parts bent outwardly for engagement with the latches hereinafterWith each of the brackets 22 a pivoted latch is adapted to engage, twoof these latches being pivotally mounted on the part B, and two on theart C. Each latch 23 has its end thickene as shown at 24, to pass downaround the corresponding bracket 22, so that when the latches are in theposition shown in Fig. 1, the parts A, B-and are prevented fromlongitudinal movement, except as a whole, bein firmly locked together,with the ends of the parts 3 fitting into corresponding grooves 111 theparts B and C. To the parts B and C are attached wheels 25, in the usualmanner, which are adapted to run on tracks 26, so that .the wholeapparatus, consisting of the parts A, B and 0 may be moved as a wholefrom one part of theplant to another, the latches being in the positionshown in Flg. 1, or whereby when the latches 23 are thrown up, the partsB and C may be separated from the retort A, whereupon the latter may berotated by means of power applied to,

the pulley 18 for a purpose hereinafter described. The part B is thefurnace portion, and is provided with a grate 26', pipe 27 for theadmission of aseous or liquid fuel, and door 28, provide? with a latch29. Of course, any desired form of fuel could be used in the part B. J

.The rear end of the part B is closed by a erforated plate 30, theperforations being lbcated 0 )posite the tubes 7 in the retort A. Aroundtins perforated plate, the rear open end of the part B is thickened, asshown at 31, and is provided with a circular groove, into which groovethe part 3carried by the retort is adapted to fit.

The part C simply serves to carry the waste products of combustion afterthey have passed through the tubes 7 of the retort into the chimney. Itconsists of a flue, preferably cylindrlcal in form, havin one endthickened, as shown at 32, said thickened end having a groove thereinfor the reception of the part 3 on one end of the retort A.

33 represents a chimney, and 34 the flue thereof.

35 represents a cylindrical o ening, into which the open aid of the partis adapted to telescope. This arrangement is adopted so that the parts Band C may be moved along the track out of engagement with the retort A,leaving the latter free to rotate.

The operation is as follows :The apparatus being in the position shownin Fig. 1, if it is desired to make as, coke, and gas retort carbon, forexamp e, the upper door of the retort is opened and a suitable charge ofsoft coal introduced into the interior of said retort into thespacebetween the pipes 7. The upper door is then firmly closed,

and connections made between the discharge pipes 10 at the top of theretort leading to the gasometer, or to any place where gas is to beused. A fire is then started in the furnace B, and the hot prodnets ofcombustion pass through the tubes 7,

distilling the coal in the retort A, the gases passing out through thedischarge pipes 10.

After this operation has been continued for a sufficient time to distillabout half of the coal, the latches 23 are disengaged from the brackets22, and the parts B and C moved along the track 20 out of contact withthe retort A. All the cocks in the pipes 10 being closed, the upperpipes are disconnected from the pi es leading to the gaso nieter, and bymeans 0 power applied to the pulley 18, the retort is rotated 180. Theparts B and C are then brought back into connection with the retort A,and the latches 23 moved down into the position shown in Fig. 1. Thepipes at the top of the retort are then connected to the gas delivepipes, and the cooks therein 0 ened. The istillation process is thencarried on to its close, and at the end the upper pipes are disconnectedfrom the gas delivery pipes, and both the upper and ower doors are"opened. By means of iron rods, the coke between the pipe 7' is forceddown, out through the lower door, leaving the ipes 7, and in fact thewhole interior of tlie retort, coated with an even layer of gas carbon.

The fact that the whole interior of the retort, including the pi s, iscoated with an even layer of gas car on, makes the retort highly usefulin the production of sodium, for example, in which it is. necessary thatthe substances under treatment should be subjected to the action ofcarbon under heat, and in which it is desirable that the retort shouldbe frequently rotated. These retorts ma be used either with or withoutcarbon an are arranged in sets so that they can be moved from one partof the plant to another.

For some of the reactions hereinafter mentioned, it is necessary to havea certain amount of carbon in the retort and for other reactions theremust be no carbon. To obtain this carbon, I charge the retort with softcoal and'heat the same, up to the distillation point, b burning gas,coke, coal, or any desired klnd of fuel in the furnace B. As the retortA becomes heated up, the gases from the fuel pass out of the upper pipes10 in the usual manner, the cooks 11 being open, which gases arecollected and either used to run another retort or stored for futureconsumption.

As described in the description of the apparatus, the retort isrevolved180 one or more times during the distillation process, so that thedeposit of gas carbon within the retort on the tubes and walls thereofmay be substantially uniform. There is left in the retort coke and adeposit of gas carbon. The former may be removed by opening the top andbottom doors 9 of the retort and pushing out the coke from between thehorizontal flues 7, leaving the deposit of gas carbon on the tubes andon the inside of the end plates and on the walls of the retort. Thisee'mse,

IL 1 'retor l may be then used where itstands'or conve ed awa.to'anot-her portion of the plant by latchin the three parts A, B and Ctogether and r easing the bearing around the rods or shafts 17. 1

The- South Carolina clays, which my process is primarily ,designed totreat (although it 18 by no means restricted to the treatment of theseclays) consist of the following arts chemically combined-A1 0 2810,,2%,0, XFe O that is to say, one

' molecule of oxid of aluminum, two molecules of silica, two moleculesof water, and 1 to 3 per cent. of ferrous or'fer'ric oxids or both,approximately stated.

After determining the amount-of alumina in the clay, I mix with one artof cla six times the amount of bi-sul ate of so ium, as compared withthe alumina in the clay, basing the weights used'upon the molecularweights of the alumina and'the bi-sulfate of sodium, so that the latter.salt may furnish enough sulfuric acid. to give up 3 molecules of saidacid to the alumina. Insplace of clay, I may, of course, use other oresof aluminum, such as bauxite or corundum,

The uantity of acid bi-sulfate of sodium used s ould, of course, besufiicient to furnish whatever iron is present with a sufficient amountof sulfuric acid, as well as the alumina, based uponthe atomic weightsof the oxids of iron and the bi-sulfate of sodium.

This mixture is then heated in one of my retorts, producing adoublesulfate of aluminum and sodium re resented by the formulaAl (S0 dNa,,Sferric alum, sulfate of sodium, and free silica, according to thefollowing reaction al o esio en xr o GNaHSO,

It should be mentioned that the a'etort should only be charged so thatit is about two-thirds full and before heating the retort "it isseparated from the furnace B and chimcombined with 1 molecule ofsulfate,of aluminum. During the same reaction silica is also formed inananhydrous condition, and when the reaction is ended, the mass assumes adirty yellowish white color. As soon as the reaction is ended, the'lower bearings of the retort A areremoved and the whole approcess.

also produced which paratus beingthen' free to move is rolled off thetrack to another portions-of the plant. The upper and lower pipes in theretort are then opened and steam. or hot waterv is passed in through thepipes at the top and -1s dis charged through the pipes at the bottom,carrying out with it the'contents of the retort. The double-sulfates aredissolved out 1 of the fused "mass, leaving the silica in an insolubleform. The mass of material obtained by washingout the retorts'is then'filtered, separating the silica, which is washed again, if necessary,and is then in a finev white condition, admirably" suited for makingglass and other purposes for which silica is commonly used.

It will be noted that sulfate of aluminum is united chemically with 3molecules of sulfate of sodium instead of with 1 molecule, as inordinary aluifi, and'by making useof thisnew double sulfate, I havedevised an im roved sodium This double sulfate is fused in one of myretorts with cr .olite in the proportions indicated by the ollowingreact-ion, no carbon being present in the retorts: .t

by my process the Fluorid of aluminum is produced, which insoluble,Sulfate of sodium is soluble. The mixture is allowed to partially cooland while; still hot is lixivi'atedand the fiuorid of aluminum separatedfrom the solution of the sulfate of sodium by filtration.. The fluoridof aluminum, after being. allowed to dry,-is heated to about rednessandshowered down upon,melted metallic sodium, whereuponthe followingreaction takes place:

This reaction results in the production.

of metallic aluminum and cryolite. A't the same time a slagis'formedqwhich may be used to fuse with the product obtained from claysafter fusing them with bi-sulfate sodium, as mentioned above.

I obtain metallic sodium as follows: Thesulfate of sodium alreadyobtained is placed in one of the retorts A, which has beenlined with gas-carbon,-as previously described.

Coke, finely pulverized, may then be added,

if necessary, and the retort is then heated, whereupon sulfid. of sodiumis produced, there still being an excessof carbon left in the retort.Caustic lime is then added and the retort heated to about 800 CL, whenmetallic sodium commences to distilover and is condensed in the usualmanner, the

reaction being as. follows cNa s+6cao+ec=cna +eqas+eod other words, Iproduce metallic sodium indirectlyv from the sulfate of sodium ordirectly from the sulfidfi I use lime to take the sulfur from thesodium, formin sodium oxid, which is immediately reducedto metallicsodium by the carbon present in the retort. I also manufacture aluminateof sodium, Al O' ,3Na O, in a similar manner; that is, I place the,double'sulfate of sodium and aluminum already obtained in one of mycarbon lined retorts, and heat it until thesulfate of aluminum isdecomposed, forming the oxid. Sulfurous acid gas is driven off, passesover carbon monoxid and dioxid into a discharge pipe, which leads into asulfuric'acid chamber, where the usuaL treatment for makingsulfuric acidtakes place.- There isleft in the retort alumina either mixed orchemically" combined with 3 molecules of'sulfid of sodium, Al Q 3Na S, I

I then add caustic lime in sufficient quan- 'tities to take up thesulfur, whereupon the following reaction takes place:

A1 0 ,3Na S+3CaO=Al;O 3Na O-l3CaS.

The aluminate of sodium thus produced is soluble while the sulfid ofcalcium is insoluble. The mass is allowed to cool and treated withwater, whereupon the aluminate of sodium dissolves and the sulfid ofcalcium canbe. separated from the solution byfiltration or decantation.

Artificial cryolite can also be made from "the aluminate of sodium soobtained by treating fluorid of calcium (fluorspar)-in a" lead tank withsulfuric acid, whereupon hydro-fluoric acid is formed, in the usualmanner, which acid is led into a solution of aluminate of sodium througha lead pipe.

The following reaction takes place:

Al O ,3 Na O+ 12HF=Al F,,6NaF+6H O. The hydro fluoric acid is rapidlycondensed and artificial cryolite is precipitated.

Carbonate of sodium may also be produced as follows: Carbonate of limeis heated in one of my retorts and the carbonic acid produced is ledaway and stored up for use: Aluminate of sodium in solution is thentreated with this gas, whereupon the hydrate of aluminum isprecipitated, while carbonate of sodium remains in solution.Whenevercarbonates or caustic alkalies. are heatedat a red heat, thedifliculty has been to keep the carbon, which is lighter than thematerial treated, always in contact with the entire mass of the meltedmaterial.

. In my retort, the gas carbon is fixed around the fines and outerportion of the re-. tort and held there immovably, according to thereactions already set forth. According and chimney to my method, anewdouble sulfate of alusilica may be produced, as ell as fluorid ofaluminum, -su fate of sodium, metallic aluminum, artificial cryolite,metallic sodium, aluminate of sodium, besides various others.

In a complete plant I design to use-one series or batter of my retortswithout distilling coal in t cm at all, and in another series, where itis desirable to, use a carbon lined retort, coal is distilled, forminggas and a fresh lining of graphite or fresh carbonat every distillation,taking care in every distilling operation to tip the getort over, sothat the bottom door is on the top and vice versa} ,The retort ispreferably suspended from above by hangin supports, the bottom halfbearings being lifted up to the shaft by bolts and screws, as shown inthe drawing. The retort is detachably fixed to the furnace connectingportions by means of cylindrical projections fitting into circulargrooves, and these with the latches support the retort A when it isreleased from its bearings, so that the whole structure, consisting ofthe three parts A, B and C may be rolled away to another part of theplant.

From the sodium aluminate made as above described, metallic sodium maybe produced in the following manner :.Sodium aluminate is placed in oneof my carbon lined retorts'which is then heated and anhydrous sodiumcarbonate constantly added. At 800 C. the alumina displaces the carbonicacid gas, and the carbon set free immediately reduces the sodium oxid asfollows The reactions are set forth below: Al O Na,O+2Na CO +2G= 1. Thehereindescribed process. of mak- -105 ing sodium, 'whichconsists inheating in a closed vessel sodium aluminate in the presence of a sodiumcompound and carbon, substantially as described.

2."The herein described process of mak- 110 ing sodium, which consistsin heating in a closed vessel sodium aluminate in the ,pres-' ence ofsodium carbonate and gas carbon, substantially as described.

In testimony whereof, I aflix my signature, 115 in presence of twowitnesses.

' PHILIP A. EMANUEL.

Witnesses:

T. A. WITHERsPoo R. M. PARKER.

